CN108190882A - Conductive graphite paper and preparation method thereof - Google Patents
Conductive graphite paper and preparation method thereof Download PDFInfo
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- CN108190882A CN108190882A CN201810161641.3A CN201810161641A CN108190882A CN 108190882 A CN108190882 A CN 108190882A CN 201810161641 A CN201810161641 A CN 201810161641A CN 108190882 A CN108190882 A CN 108190882A
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Abstract
The present invention relates to a kind of preparation methods of conductive graphite paper, include the following steps：Crystalline flake graphite with concentrated sulfuric acid solution is mixed, obtains the first mixture；Oxidant is added in into first mixture, carries out oxidation intercalation, obtains the second mixture；Second mixture is washed, obtains prefabrication；The prefabrication is placed in a chamber, first the chamber is vacuumized, then inert gas is passed through into the chamber, and carries out high-temperature expansion processing, obtains expanded graphite meterial；And rolling at least once is carried out to the expanded graphite meterial, obtain conductive graphite paper.The present invention also provides a kind of conductive graphite paper.
Description
Technical field
The present invention relates to grapheme materials more particularly to a kind of conductive graphite paper and preparation method thereof.
Background technology
Since 2010, conductive graphite paper is prepared by raw material batch of Delanium, and as electrical and electronic product
Cooling application.Later, with the raising of the power of electronic product, people begin to use the Delanium graphite paper of high thermal conductivity coefficient
(thermal conductivity is in more than 1500W/mk), for the height of the consumer electronics products such as flat panel TV, smart mobile phone, laptop
Effect heat dissipation.But the cost that conductive graphite paper is prepared into using Delanium as raw material is higher.
Then, for cost consideration, people start to consider to replace part Delanium using native graphite.It is however, existing
The thermal conductivity of thermal paper manufactured out using native graphite as raw material is relatively low (280W/mk~300W/mk), is also difficult to reach
The technology application requirement of fast-developing high power electronic product till now.
Invention content
In view of this, it is necessory to provide it is a kind of can be used for the extensive conductive graphite paper for preparing excellent thermal conductivity and its
Preparation method.
The present invention provides a kind of preparation method of conductive graphite paper, includes the following steps：By crystalline flake graphite and the concentrated sulfuric acid
Solution mixes, and carries out oxidation reaction, obtains the first mixture, wherein, the mass ratio of the crystalline flake graphite and concentrated sulfuric acid solution is
1:(2.5~3.0), the mass fraction of sulfuric acid is 95%~98% in the concentrated sulfuric acid solution；Add into first mixture
Enter oxidant, carry out oxidation intercalation, obtain the second mixture, wherein the intercalator is sulfuric acid and salpeter solution, it is described
The mass ratio of salpeter solution and the crystalline flake graphite is 1:5~1:10, the mass fraction of nitric acid is 50% in the salpeter solution
~68%；Second mixture is washed, obtains prefabrication；The prefabrication is placed in a chamber, first to described
Chamber vacuumizes, then inert gas is passed through into the chamber, and carries out high-temperature expansion processing, obtains expanded graphite meterial；With
And rolling at least once is carried out to the expanded graphite meterial, obtain conductive graphite paper.
The present invention also provides the conductive graphite paper that a kind of method is prepared, the sulfur content of the conductive graphite paper is less than
1500ppm, the thermal conductivity of the conductive graphite paper is 400W/ (mK)~600W/ (mK).
Compared with prior art, the preparation method of the conductive graphite paper has the following advantages：
First, relative to the prior art scale for cost is higher, is used as raw material using high-carbon graphite in the application
For graphite as raw material, cost is relatively low.Second, crystalline flake graphite concentrated sulfuric acid solution, salpeter solution are subjected to oxidation reaction respectively
And intercalation, then handled via high-temperature expansion, you can so that graphite realizes expansion.The expansion process raw material of the conductive graphite paper
Only concentrated sulfuric acid solution, salpeter solution, technique is simpler, easily operated.Third in high-temperature expansion processing procedure, is first taken out
Vacuum so that the chamber forms vacuum tightness tiny structure, then is passed through inert gas into the chamber, with the expansion to graphite
Process carries out the protection of inert atmosphere, meanwhile, the pernicious gas that also graphite can be facilitated to be discharged in expansion process discharges chamber as early as possible
Body.
Further, by multiple rolling, and the heat conduction can be increased using flat tripe rolling in last time roll milling process
The surface smoothness of graphite paper.Also, the obtained higher (400W/ (mK)~600W/ (m of the heat transfer efficiency of conductive graphite paper
K)), thus can be directly used in the fields such as radiating electronic element.
Description of the drawings
Fig. 1 and Fig. 2 is the scanning electron microscope (SEM) photograph of 1 obtained expanded graphite meterial of the embodiment of the present invention；
Fig. 3 is the photo of 1 obtained conductive graphite paper of the embodiment of the present invention；
Fig. 4 is the scanning electron microscope (SEM) photograph of 1 obtained expanded graphite meterial of comparative example.
Specific examples below will be further illustrated the present invention with reference to above-mentioned attached drawing.
Specific embodiment
Conductive graphite paper provided by the invention and preparation method thereof is described further below with reference to attached drawing.
The present invention provides a kind of preparation method of conductive graphite paper.The preparation method includes the following steps：
S1 mixes crystalline flake graphite with concentrated sulfuric acid solution, carries out oxidation reaction, obtains the first mixture, wherein, the squama
The mass ratio of piece graphite and concentrated sulfuric acid solution is 1:(2.5~3.0), the mass fraction of sulfuric acid is 95% in the concentrated sulfuric acid solution
~98%；
S2 adds in oxidant into first mixture, carries out oxidation intercalation, obtains the second mixture, wherein
The oxidant is salpeter solution, and the mass ratio of the salpeter solution and the crystalline flake graphite is 1:5~1:10, the nitric acid is molten
The mass fraction of nitric acid is 50%~68% in liquid；
S3 washes second mixture, obtains prefabrication；
The prefabrication is placed in a chamber by S4, and first the chamber is vacuumized, then is passed through inertia into the chamber
Gas, and high-temperature expansion processing is carried out, obtain expanded graphite meterial；
S5 carries out rolling at least once to the expanded graphite meterial, obtains conductive graphite paper.
In step sl, the concentrated sulfuric acid solution and the crystalline flake graphite can be placed in a mixing machine, are uniformly mixed.It should
The purpose of step is to do premise preparation for the oxidation intercalation of step S2.The incorporation time is 15 minutes~30 points
Clock, temperature is 20 DEG C~25 DEG C during being somebody's turn to do.
In a preferred embodiment, the mass ratio of the crystalline flake graphite and concentrated sulfuric acid solution is 1:2.5, the concentrated sulfuric acid
The mass fraction of sulfuric acid is 98% in solution.
The crystalline flake graphite is the mineral raw material directly exploited.The crystalline flake graphite is used as raw material, adds without additional
Work.The size and phosphorus content of the crystalline flake graphite do not limit.
In step s 2, it is easier by the layer of step S1 concentrated sulfuric acid solutions treated crystalline flake graphite with layer by intercalation.
The time of the oxidation intercalation is 60 minutes~90 minutes, and the temperature of the intercalation is below 70 DEG C.
Further, in intercalation, start to be stirred the first mixture, later, a period of time is stood, in order to better
Aoxidize intercalation.
In a preferred embodiment, the mass ratio of the salpeter solution and the crystalline flake graphite is 1:5, the nitric acid is molten
The mass fraction of nitric acid is 68% in liquid.
In step s3, second mixture is washed, until pH value is 6~7.
In step s 4, it in high-temperature expansion processing procedure, first vacuumizes so that it is micro- negative that the chamber forms vacuum tightness
Pressure, then inert gas is passed through into the chamber, to carry out the protection of inert atmosphere to the expansion process of graphite, meanwhile, also may be used
The pernicious gas that graphite is discharged in expansion process is facilitated to discharge cavity as early as possible.The prefabrication passes through high-temperature expansion, can obtain
Expanded graphite meterial.Compared with raw material crystalline flake graphite, the swelling volume of the expanded graphite meterial is about the volume of crystalline flake graphite
80~140 times.
The time of the high-temperature expansion processing is 5 seconds~10 minutes.The temperature of the high-temperature expansion processing is 800 degrees Celsius
~1000 degrees Celsius.
During the high-temperature expansion processing, continue to be passed through inert gas, the pressure of the chamber into the chamber
For 10torr~15torr, the rate that is passed through of the inert gas is 3 × 106Standard milliliters/minute~5 × 106Standard milliliters/
Minute.The volume ratio of mixed gas of the inert gas for nitrogen and argon gas, the nitrogen and argon gas is 95:5~90:10.
In step s 5, the number of the rolling is 5~8 times, and flat tripe rolling is used during last time rolling.
Due to by multiple rolling, and the conductive graphite paper can not only be increased using flat tripe rolling in last time roll milling process
Surface smoothness and graphite paper brightness, and the consistency of thickness of graphite paper can be made relatively good.
The present invention also provides a kind of conductive graphite paper.The conductive graphite paper is is prepared using the above method.It is described to lead
The sulfur content of hot graphite paper is less than 1500ppm, and the thermal conductivity of the conductive graphite paper is 400W/ (mK)~600W/ (mK).
The thickness of the conductive graphite paper is 200 microns~500 microns.
Hereinafter, it will further illustrate in conjunction with specific embodiments.
Embodiment (1)
The preparation method of conductive graphite paper includes the following steps described in the embodiment：
(1) graphite ore is obtained into crystalline flake graphite by purification, crushing.Crystalline flake graphite with concentrated sulfuric acid solution is placed in and is mixed
15 minutes in machine, wherein the quality of crystalline flake graphite is 150 ± 5Kg, and the quality of concentrated sulfuric acid solution is 378 ± 5Kg, and sulfuric acid concentration is
98%.
(2) it in the salpeter solution injection mixing machine for being about 58% by 30 ± 0.5Kg mass fractions, stirs 30 minutes, stands
60 minutes, obtain the second mixture.
(3) second mixture is washed, until pH value is 6~7, it is dry, obtain prefabrication.
(4) prefabrication is placed in chamber, first the chamber is vacuumized, then body is continually fed into the chamber
Product is than being 95:The inert gas of 5 nitrogen and helium composition.The rate that is passed through of the inert gas is 3 × 106Standard milliliters/
Minute.The indoor air pressure of chamber at this time is 10torr.The chamber temp is risen to 1000 degrees Celsius in advance, and holding 10 is small
When, graphite is sent into chamber to carry out high-temperature expansion processing later, puffing time is 7 seconds, obtains expanded graphite meterial.
(5) 6 rollings are carried out to obtained expanded graphite meterial, also, using flat during last time rolling
Tripe rolling obtains conductive graphite paper.
To the obtained expanded graphite meterial of step (4) in embodiment (1) carry out Morphology analysis, the result is shown in Figure 1 and
Fig. 2.
It takes pictures to obtained conductive graphite paper in embodiment (1), as a result sees Fig. 3.
In order to better illustrate the excellent performance of the conductive graphite paper of the present embodiment (1), the present invention also provides a comparative examples
(1)。
The preparation method of comparative example (1) the conductive graphite paper includes the following steps：
(1) high-carbon graphite that phosphorus content is 99% is provided.By high-carbon graphite and concentrated sulfuric acid solution with 1:2 mass ratio is placed in
15 minutes in mixing machine, the concentrated sulfuric acid solution mass fraction is about 98%.
(2) 35% hydrogen peroxide is sprayed again, and the hydrogen peroxide of sprinkling and the mass ratio of high-carbon graphite are 0.125:1.Stirring
20min stands 20min.
(3) hydrofluoric acid solution that mass fraction is 40% is added in, stirs 30min, stands 30min.Hydrofluoric acid solution with
The mass ratio of high-carbon graphite is 0.165:1.
(4) 7~8 times of water are added in, are repeatedly washed, until supernatant pH is 3~7.
(5) high-temperature expansion is carried out, bulking equipment chamber indoor temperature is upgraded to 1000 degrees Celsius in advance, and the retention time is 10
Hour, the composition of atmosphere is air wherein in expansion process, and Bulking Time 7s is passed through air into chamber by air blower,
The flow for being passed through air is 10m3/min。
(6) 6 rollings are finally carried out, last time rolling is bulging rolling.
Morphology analysis is carried out to the obtained expanded graphite meterial of step (5) in comparative example (1), as a result sees Fig. 4.
By Fig. 1, Fig. 2, Fig. 4 as it can be seen that relative to for comparative example (1), the obtained expanded graphite material of the present embodiment (1)
The expansion multiple of material is higher, more fluffy between adjacent carbon-coating.
As seen from Figure 3, the obtained conductive graphite paper of the present embodiment (1) is relatively smooth smooth.
Further, the thermal conductivity and expanded graphite meterial of conductive graphite paper obtained to embodiment (1) and comparative example (1)
Sulfur content tested, the results are shown in Table 1.
Table 1
| Embodiment (1) | Comparative example (1) | |
| The sulfur content (ppm) of expanded graphite meterial | 1400 | 2300 |
| Thermal conductivity (the W/ (mK) of conductive graphite paper | 403 | 323 |
By table 1 as it can be seen that for comparative example (1), the sulfur content of embodiment (1) described expanded graphite meterial is less,
Thermal conductivity is higher, this further demonstrates the obtained conductive graphite paper of the application with fabulous application prospect.
Embodiment (2)
The preparation method of conductive graphite paper includes the following steps described in the embodiment：
(1) graphite ore is obtained into crystalline flake graphite by purification, crushing.Crystalline flake graphite with concentrated sulfuric acid solution is placed in and is mixed
10 minutes in machine, wherein the quality of crystalline flake graphite be 150 ± 5Kg, the matter for the concentrated sulfuric acid solution that the mass fraction is about 95%
It measures as 420 ± 5Kg.
(2) it in the salpeter solution injection mixing machine for being about 68% by 20 ± 0.5Kg mass fractions, stirs 30 minutes, stands
50 minutes, obtain the second mixture.
(3) second mixture is washed, until pH value is 6~7, it is dry, obtain prefabrication.
(4) prefabrication is placed in chamber, first the chamber is vacuumized, then body is continually fed into the chamber
Product is than being 90:The inert gas of 10 nitrogen and helium composition.The rate that is passed through of the inert gas is 3 × 106Standard milliliters/
Minute.The indoor air pressure of chamber at this time is 12torr.The temperature of the chamber is risen to 900 degrees Celsius, and is kept for 10 hours, later
Graphite is sent into chamber to carry out high-temperature expansion processing, puffing time is 5 seconds, obtains expanded graphite meterial.
(5) 7 rollings are carried out to obtained expanded graphite meterial, also, using flat during last time rolling
Tripe rolling obtains conductive graphite paper.
Embodiment (3)
The preparation method of conductive graphite paper includes the following steps described in the embodiment：
(1) graphite ore is obtained into crystalline flake graphite by purification, crushing.Crystalline flake graphite with concentrated sulfuric acid solution is placed in and is mixed
20 minutes in machine, wherein the quality of crystalline flake graphite be 150 ± 5Kg, the matter for the concentrated sulfuric acid solution that the mass fraction is about 95%
It measures as 450 ± 5Kg.
(2) it in the salpeter solution injection mixing machine for being about 62% by 10 ± 0.5Kg mass fractions, stirs 40 minutes, stands
40 minutes, obtain the second mixture.
(3) second mixture is washed, until pH value is 6~7, it is dry, obtain prefabrication.
(4) prefabrication is placed in chamber, first the chamber is vacuumized, then body is continually fed into the chamber
Product is than being 95:The inert gas of 5 nitrogen and helium composition, the rate that is passed through of the inert gas is 3 × 106Standard milliliters/
Minute.The indoor air pressure of chamber at this time is 15torr.When bulking equipment chamber indoor temperature being upgraded to 1050 degrees Celsius in advance, and being kept
Between for 10 hours, graphite is sent into chamber to carry out high-temperature expansion processing later, puffing time is 5 seconds, obtains expanded graphite material
Material.
(5) 8 rollings are carried out to obtained expanded graphite meterial, also, using flat during last time rolling
Tripe rolling obtains conductive graphite paper.
The explanation of above example is only intended to facilitate the understanding of the method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvement and modification are also fallen within the protection scope of the claims of the present invention.
The foregoing description of the disclosed embodiments enables professional and technical personnel in the field to realize or use the present invention.
A variety of modifications of these embodiments will be apparent for those skilled in the art, it is as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one
The most wide range caused.
Claims (10)
1. a kind of preparation method of conductive graphite paper, which is characterized in that it includes the following steps：
Crystalline flake graphite with concentrated sulfuric acid solution is mixed, obtains the first mixture, wherein, the crystalline flake graphite and concentrated sulfuric acid solution
Mass ratio is 1:(2.5~3.0), the mass fraction of sulfuric acid is 95%~98% in the concentrated sulfuric acid solution；
Oxidant is added in into first mixture, carries out oxidation intercalation, obtains the second mixture, wherein the oxidation
Agent is salpeter solution, and the mass ratio of the crystalline flake graphite and salpeter solution is 1:5~1:10, the matter of nitric acid in the salpeter solution
It is 50%~68% to measure score；
Second mixture is washed, obtains prefabrication；
The prefabrication is placed in a chamber, first the chamber is vacuumized, then inert gas is passed through into the chamber, and
High-temperature expansion processing is carried out, obtains expanded graphite meterial；And rolling at least once is carried out to the expanded graphite meterial, it obtains
Conductive graphite paper.
2. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the incorporation time for 15 minutes~
30 minutes, the temperature of the oxidation reaction was 20 DEG C~25 DEG C.
3. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the time of the oxidation intercalation
It it is 60 minutes~90 minutes, the temperature of the oxidation intercalation is below 70 DEG C.
4. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that water is carried out to second mixture
It washes, until pH value is 6~7.
5. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the time of the high-temperature expansion processing
It it is 5 seconds~10 minutes, the temperature of the high-temperature expansion processing is 800 degrees Celsius~1000 degrees Celsius.
6. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the process of the high-temperature expansion processing
In, continue to be passed through inert gas into the chamber, the pressure of the chamber is 10torr~15torr, the inert gas
It is 3 × 10 to be passed through rate6Standard milliliters/minute~5 × 106Standard milliliters/minute.
7. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the inert gas is nitrogen and argon
The volume ratio of the mixed gas of gas, the nitrogen and argon gas is 95:5~90:10.
8. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the number of the rolling is 5~8
It is secondary, flat tripe rolling is used during last time rolling.
It is 9. a kind of using the conductive graphite paper being prepared such as any one of claim 1~8 the method, which is characterized in that institute
The sulfur content for stating conductive graphite paper is less than 1500ppm, and the thermal conductivity of the conductive graphite paper is 400W/ (mK)~600W/
(m·K)。
10. the preparation method of conductive graphite paper as described in claim 1, which is characterized in that the thickness of the conductive graphite paper
It is 200 microns~500 microns.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109133923A (en) * | 2018-08-21 | 2019-01-04 | 大同新成新材料股份有限公司 | A kind of method that graphene oxide-special graphite powder prepares special graphite paper |
| CN109437952A (en) * | 2018-11-30 | 2019-03-08 | 大同新成新材料股份有限公司 | A kind of method that C/C composite prepares graphite paper |
| CN111924837A (en) * | 2020-08-24 | 2020-11-13 | 山东众弘新材料有限公司 | Preparation method of high-purity graphite paper |
| CN112408371A (en) * | 2020-10-30 | 2021-02-26 | 宁波石墨烯创新中心有限公司 | Graphene heat-conducting film, preparation method thereof and electronic equipment |
| CN115959657A (en) * | 2023-03-16 | 2023-04-14 | 清华大学 | Natural graphite-based heat dissipation film and preparation method thereof |
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| CN115959657A (en) * | 2023-03-16 | 2023-04-14 | 清华大学 | Natural graphite-based heat dissipation film and preparation method thereof |
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Application publication date: 20180622 |